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Ammonia → 3-Fluoro-5-nitrobenzamide

HRID 522912
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인쇄 미리보기

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HRID 522912 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)[C:5]#[N:6].O.S(=O)(=O)(O)[OH:15].N>C(O)(C(F)(F)F)=O>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)[C:5]([NH2:6])=[O:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 962WaterHCID 1118Sulfuric AcidHCID 27590493-Fluoro-5-nitrobenzonitrile

생성물 1

HCID 509984493-Fluoro-5-nitrobenzamide수율 36%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

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온도
70 °C

실험 절차

To a solution of 3-fluoro-5-nitrobenzonitrile (1.0 g, 6.02 mmoL) in TFA (8 mL) was added water (1 mL) and conc. sulfuric acid (2 mL). The reaction mixture was heated to 70° C. and stirred for 24 h. Then the reaction mixture was cooled to 0° C. and liquid ammonia solution was added. The solidified solid was filtered through Celite® (diatomaceous earth) and washed with water to obtain 3-fluoro-5-nitrobenzamide (0.400 g, 36%) as an off white solid. Observed mass (M−1): 183.02.

후처리

  1. temperatureThen the reaction mixture was cooled to 0° C.
  2. filtrationThe solidified solid was filtered through Celite® (diatomaceous earth)
  3. washwashed with water

출처 및 근거

ORD 기록
ord-04ae21c41fc443d5a63b8c3e6ca43f55
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09334269B2

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